Extended length tube structures

ABSTRACT

An extended length tube structure includes a first ceramic tube segment having a first end and a second end, and a second ceramic tube segment having a first end and a second end, in which the second end of the first ceramic tube segment is arranged to face the first end of the second ceramic tube segment. A ceramic coupling component is positioned to circumscribe the end-to-end configuration of the tube segments, and is sinter-bonded to the tube segments to form a continuous, extended length tube structure having a seal, such as a sinter bond or an interference bond, that is free of bond materials.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation of U.S. patent application Ser. No.13/849,354 entitled “EXTENDED LENGTH TUBE STRUCTURES,” by Lawrence M.Banach et al., filed Mar. 22, 2013, which claims priority under 35U.S.C. § 119(e) to U.S. Patent Application No. 61/614,499 entitled“EXTENDED LENGTH TUBE STRUCTURES,” by Lawrence M. Banach et al., filedMar. 22, 2012, both of which applications are assigned to the currentassignee hereof and incorporated herein by reference in theirentireties.

FIELD OF THE DISCLOSURE

This disclosure, in general, relates to extended-length tube structures,and more particularly, to ceramic tube structures joined together bysinter bonds.

BRIEF DESCRIPTION OF THE INVENTION

Embodiments of the present invention are generally drawn toextended-length tube structures, formed as ceramic materials,particularly including silicon carbide-based materials. Embodiments ofextended length tube structure of the present invention generallyinclude a first tube segment and a second tube segment joined togetherby a ceramic coupling component. The first tube segment has first andsecond ends, the second tube segment has first and second ends, and thetwo segments are arranged in an end-to-end configuration such that thesecond end of the first ceramic tube segment and the first end of thesecond tube segment face each other. The ceramic coupling componentserves to bond the first and second tube segments together, and ispositioned so as to be sinter-bonded to the second end of the first tubesegment and to the first end of the second tube segment. In particular,the ceramic coupling component is positioned to circumscribe theend-to-end configuration of the tube segments, and is sinter-bonded tothe tube segments to form an continuous, extended length, tube structurehaving a seal, such as a sinter bond or an interference bond, free ofbond materials.

BRIEF DESCRIPTION OF THE DRAWINGS

The present disclosure may be better understood, and its numerousfeatures and advantages made apparent to those skilled in the art byreferencing the accompanying drawings.

FIG. 1 shows a cross-section of an extended length tube structureaccording to an embodiment of the present invention, in which tubestructures are abutted end-to-end and joined to each other by a ceramiccoupling component and a sinter bond therebetween.

FIG. 2 shows a plan view of the extended length tube structureembodiment shown in FIG. 1.

FIG. 3 shows an exploded plan view of the end faces of adjacent tubesegments to be abutted together according to an embodiment of thepresent invention.

FIG. 4 shows an exploded cross-section view of the end faces of adjacenttube segments of another embodiment, in which the adjacent tube segmentshave complementary L-shaped end faces.

FIG. 5 shows the sinter-bond interface between a pre-sintered siliconcarbide segment and a ceramic coupling component.

FIG. 6 shows a graph of a pressure test of one embodiment of a ceramicarticle at 200 psi.

FIG. 7 shows a graph of a pressure test at 20° C. of three embodimentsof a ceramic article.

FIG. 8 shows a graph of a pressure test at 1000° C. of the threeembodiments of FIG. 7.

FIG. 9 shows a graph of pressure vs. temperature of a pressure test ofan embodiment of a ceramic article through five (5) thermal cycles.

FIG. 10 shows a graph of a pressure test at 20° C. of three embodimentsof a ceramic article.

FIG. 11 shows a graph of a pressure test at 1000° C. of the threeembodiments of FIG. 10.

FIG. 12 shows a graph of pressure vs. temperature of a long durationtest of three embodiments of a ceramic article.

The use of the same reference symbols in different drawings indicatessimilar or identical items.

DETAILED DESCRIPTION

Embodiments of the present invention are generally drawn toextended-length tube structures, formed as ceramic materials,particularly including silicon carbide-based materials. Large-sized,such as high thermal mass and/or extended dimension bodies are difficultto manufacture as monolithic ceramic parts. Typically, extendeddimensions have notable challenges in terms of sourcing appropriatefurnaces, have high thermal budgets, and have extended andslowly-ramping sinter and anneal times. Consequently, certain structuresare made in segmented form and joined together.

According to an embodiment of the present invention, extended lengthtube structure is provided that includes a first tube segment and asecond tube segment joined together by a ceramic coupling component. Thefirst tube segment has first and second ends, the second tube segmenthas first and second ends, and the two segments are arranged in anend-to-end configuration such that the second end of the first ceramictube segment and the first end of the second tube segment face eachother. The ceramic coupling component serves to bond the first andsecond tube segments together, and is positioned so as to besinter-bonded to the second end of the first tube segment and to thefirst end of the second tube segment. The ceramic coupling component maycircumscribe the first and second tube segments at a portion on thesegments where they meet each other. Notably, the tube segments form aseal with the coupling component, a Shear Strength of the seal being notless about 25 MPa, not less than about 40 MPa, not less than about 50MPa, not less than about 75 MPa, not less than about 100 MPa, not lessthan about 100 MPa, not less than about 120 MPa, not less than about 140MPa, not less than about 170 MPa, or not less than about 200 MPa. In oneembodiment, the interface between the tube and the base componentexhibits a Shear Strength not greater than about 1000 MPa, such as notgreater than about 700 MPa, not greater than about 500 MPa, or notgreater than about 300 MPa.

As used herein, reference to Shear Strength as a particular ShearStrength value is measured by testing a sample having standardizeddimensions under load. In particular, the Shear Strength is measured bypreparing and testing a standardized sample as follows. The sample isprepared from a ceramic tube and a ceramic ring, each having a length of76.2 mm. The ceramic tube has an outer diameter (OD_(t)) of 14 mm and aninner diameter (ID_(t)) of 11 mm. The ceramic ring has an outer diameter(OD_(r)) of 20 mm, and an inner diameter (ID_(r)) of 14 mm. The ceramicring is placed around the ceramic tube so that the ends of each areflush, and the tube-ring assembly is then co-sintered. After cooling, across-sectional center segment is sliced from the sintered assembly andthickness grinded to a final thickness (t) of 3 mm. The center segmentcomprises an inner ring sliced from the ceramic tube and an outer ringsliced from the ceramic ring. The area of contact between the inner andouter rings represents the total bond area (A_(b)), and is calculatedaccording to the following formula:

A _(b) =π·OD _(t) ·t  (Formula I)

The Shear Strength of the center segment sample is tested at roomtemperature using an Instron 8562 using a 100 kN load cell at a speed of0.05 mm/min, which applies equal but opposing force to the inner andouter rings, respectively. The magnitude of the applied force isgradually increased until the rings break apart. The force (F) requiredto break the rings apart is measured in Newtons. The Shear Strengthvalue is obtained according to the following formula:

τ=F·A _(b)·10⁶  (Formula II)

It should be understood that ceramic articles as described herein can bea wide variety of dimensions and overall sizes, but the Shear Strengthvalues are based on a standardized geometry and testing approach asdescribed above. Consequently, validating the Shear Strength of a samplehaving differing dimensions larger or smaller than the standardizedsample described above requires the fabrication of a standardized sampleunder identical compositional and processing conditions to that of thesample having differing dimensions.

The ceramic tube segments may be formed by various techniques, such asform molding, slip casting, machining, isopressing, extrusion, and othershape forming techniques. However, embodiments of the present inventionare particularly drawn to large-scale tubes, typically having an outsidediameter greater than 7-9 inches, and lengths on the order of 0.5 to 3meters and above. Consequently, extruded tubes tend not to be practical,and various shape forming techniques have their practical limitations.Accordingly, various embodiments are formed by isopressing. Indeed, theextended length tube structures may have an aspect ratio defined as theratio of length (L) to outer diameter (OD) of not less than 10:1, suchas not less than about 20:1, such as not less than about 30:1, or notless than about 40:1. Since there is an ultimate limit on the length ofsuch tubes relative to diameter, most embodiments will not exceed anaspect ratio of 300:1.

According to a particular embodiment, the second end of the first tubesegment is in abutting contact with the first end of the second ceramictube segment. The end faces may have various configurations, includingsimple, planar structures, but also including complementary structuresthat “key” together when in abutting contact. One of example of thiskeyed relationship or interconnected relationship is through use of ashiplapped joint, in which facing surfaces have complementary L-shapedouter contours, as shown in a cross-sectional view, such that theyinterlock each other. In the case of planar end faces, they may beoriented in a plane perpendicular to the longitudinal access of the tubesegments, or alternatively, be oriented off-angle at some acute anglerelative to the access smaller than 90°, resembling an offcut tubestructure, such as a quill pen or hypodermic needle. In such a case, thetube segments would be oriented such that the off-angle faces arecomplementary to one another.

As mentioned briefly above, the ceramic tube segments may be formed of aceramic material, most notably silicon carbide. Additionally, thecoupling components may be formed of a ceramic material, notably siliconcarbide. The ceramic tube segments and the coupling components maycomprise silicon carbide, and in certain embodiments compriseprincipally silicon carbide, such that silicon carbide is the majoritycompositional species of the tube, typically greater than at least about70 wt %, such as greater than at least about 80 wt %, or greater than atleast about 90 wt %. In another embodiment, the tube may comprisesilicon carbide in an amount greater than at least about 91 wt %, suchas greater than at least about 99.85 wt %.

One particular form of silicon carbide is used according to certainembodiments, known as HEXOLOY®-brand silicon carbide (manufactured bySaint-Gobain Advanced Ceramics Corporation of Worcester, Mass., USA),described in U.S. Pat. No. 4,179,299 incorporated herein by reference.Suitable silicon carbides generally contain silicon carbide in an amountgreater than at least about 91 wt %, such as greater than at least about99.85 wt %, up to about 5.0 wt % carbonized organic material, from atleast about 0.15 wt % to not greater than about 3.0 wt % boron, and upto about 1.0 wt % additional carbon. The “carbonized organic material”is free carbon or uncombined carbon produced in situ by thecarbonization of the organic material used as a raw material in theprocess of forming the ceramic tube. The carbonizable organic materialsthat can be used in forming the ceramic tube include but are not limitedto phenolic resin, coal tar pitch, polyphenylene, orpolymethylphenylene.

Sintered ceramic bodies of silicon carbide according to an embodimentmay be characterized by a predominantly equiaxed microstructure, meaningthe presence of grains having an aspect ratio of less than 3:1 (i.e.,the ratio of the maximum dimension of the grains of the crystalmicrostructure to the minimum dimension of the grains of the crystalmicrostructure is less than 3:1). Moreover, the silicon carbidecomprises at least about 95 wt %, such as at least about 99 wt %alpha-phase, non-cubic crystalline silicon carbide.

The density of silicon carbide according to an embodiment is at leastabout 2.40 g/cm³, such as at least about 2.90 g/cm³, or at least about3.05 g/cm³.

According to certain embodiments, the first and second tube segments, aswell as the coupling component are all coaxial. Additionally, thecoupling component can take on any one of various outer contours, but itis generally desirable that the coupling component have an inner contourmatching the outer contour of the second end of the first tube segmentand the first end of the second tube segment. This inner contour of tubesegment is generally cylindrical, having a generally circularcross-sectional shape. The outer contour can vary, but for ease offabrication and for predictable shrinkage rates, the outer contour ofthe coupling may also be cylindrical. According to one particularfeature of an embodiment, an inner face between the coupling componentand each of the tubes segments to which it is bonded forms a seal, thatseals characterized by Shear Strength of the seal being not less about25 MPa, not less than about 40 MPa, not less than about 50 MPa, not lessthan about 75 MPa, not less than about 100 MPa, not less than about 100MPa, not less than about 120 MPa, not less than about 140 MPa, not lessthan about 170 MPa, or not less than about 200 MPa. In one embodiment,the interface between the tube and the base component exhibits a ShearStrength not greater than about 1000 MPa, such as not greater than about700 MPa, not greater than about 500 MPa, or not greater than about 300MPa.

A Nitrogen Seal Performance is determined according to a nitrogen sealperformance test, wherein nitrogen is applied at an interface of a sealat a given initial positive pressure, and pressure loss is measured by apressure gauge. Nitrogen Seal Performance is then the percent pressuredrop occurring across the seal interface over a period of 2 hours at anapplied gauge pressure of 200 psi. Embodiments herein achieve a Nitrogenseal performance of not greater than 10%, not greater than 9%, notgreater than 8%, not greater than 7%, not greater than 6%, not greaterthan 5%, not greater than 4%, not greater than 3%, not greater than 2%,not greater than 1.9%, not greater than 1.8%, not greater than 1.7%, notgreater than 1.6%, not greater than 1.5%, not greater than 1.4%, notgreater than 1.3%, not greater than 1.2%, not greater than 1.1%, notgreater than 1.0%, not greater than 0.9%, not greater than 0.8%, notgreater than 0.7%, not greater than 0.6%, not greater than 0.5%, notgreater than 0.4%, not greater than 0.3%, not greater than 0.2%, or notgreater than 0.1% of an initial pressure differential of 200 PSI (gaugepressure).

A Helium Seal Performance is determined according to a helium sealperformance test, wherein helium is applied at an interface of a seal ata given initial positive pressure and pressure loss is measured by apressure gauge. Helium Seal Performance is achieved if the pressure dropoccurring across the seal interface over a period of 2 hours is notgreater than 10%, not greater than 9%, not greater than 8%, not greaterthan 7%, not greater than 6%, not greater than 5%, not greater than 4%,not greater than 3%, not greater than 2%, not greater than 1.9%, notgreater than 1.8%, not greater than 1.7%, not greater than 1.6%, notgreater than 1.5%, not greater than 1.4%, not greater than 1.3%, notgreater than 1.2%, not greater than 1.1%, not greater than 1.0%, notgreater than 0.9%, not greater than 0.8%, not greater than 0.7%, notgreater than 0.6%, not greater than 0.5%, not greater than 0.4%, notgreater than 0.3%, not greater than 0.2%, or not greater than 0.1% of aninitial pressure differential of 87 PSI (gauge pressure)), an initialpressure differential of about 200 psi (about 13.8 bar), or an initialpressure differential of about 6 barg (bar gauge).

A Vacuum Seal Performance is determined according to a vacuum sealperformance test. In the vacuum seal performance test, a vacuum isapplied to a seal. The nitrogen gas atmosphere inside the tube is thenlowered from 1 ATM (760 torr) to a pressure of 10 torr thereby having apressure differential of 750 torr. Vacuum Seal Performance is achievedif the gain inside the tube occurring across the seal interface over aperiod of 2 hours is not greater than 10%, not greater than 9%, notgreater than 8%, not greater than 7%, not greater than 6%, not greaterthan 5%, not greater than 4%, not greater than 3%, not greater than 2%,not greater than 1.9%, not greater than 1.8%, not greater than 1.7%, notgreater than 1.6%, not greater than 1.5%, not greater than 1.4%, notgreater than 1.3%, not greater than 1.2%, not greater than 1.1%, notgreater than 1.0%, not greater than 0.9%, not greater than 0.8%, notgreater than 0.7%, not greater than 0.6%, not greater than 0.5%, notgreater than 0.4%, not greater than 0.3%, not greater than 0.2%, or notgreater than 0.1% of the pressure differential (750 torr).

In each of the seal performance tests, the bond or interface issubjected to the above-described pressure differential. Depending on thegeometry of the part, an inner volume is pressurized or evacuated, andholes plugged. In a case of an external seal, such as in the case of aflange on a tube, an end-cap is positioned to cover the flange andexposed bore of the tube, the cap being offset from the bore to allowfluid communication (and hence pressure/vacuum) extending radially up tothe bond region. Caps/plugs can have varying geometries to fit the partundergoing test, and can be sealed with a vacuum grease to ensure apressure tight, hermetic seal.

Sintered ceramic articles as described herein can be formed through amulti-step sintering approach. For example, a green ceramic tube isformed through any one of suitable shape forming technologies, such asmolding, slip casting, isopressing, machining, and particularlyextrusion. As is generally understood in the art, the green ceramic tubegenerally contains a water or organic liquid phase combined with variousprocessing aids and binders. For additional information on compositionaldetails, reference can be made to U.S. Pat. No. 4,179,299 incorporatedherein by reference.

Extended length tube structures according to embodiments here and may beformed by various techniques. According to one, the first and secondtube segments are provided, each having first and second ends. Each ofthe first and second tube segments are pre-sintered, at a temperatureabove 2000° C., such as above 2050° C., but generally below 2400° C.,such as below 2300° C., such as below 2250° C. A suitable target rangefor sintering the green ceramic tube in the case of silicon carbide canlie within a range of 2100−2200° C. Sintering times can vary, and arelargely dependent on the thermal mass of the tube. However, typicallysintering times range from 15 minutes to 10 hours, such as not less thanabout 30 minutes, such as not less than about 1 hour, such as not lessthan about 1.5 hours. While large, high mass tubes may require extendedsintering times, typically sintering times do not exceed 30 hours, suchas not great than 20 hours, such as not greater than 10 hours.

After the sintering step is completed, at least a portion of an outersurface of the sintered tube is subjected to surface cleaning.Typically, at least the portion of the tube that will contact the basecomponent will be subjected to surface cleaning. In this respect, it hasbeen found that the outer surface of the tube can carry contaminates,such as contaminates that are deposited during the sintering process, orwhich form as a consequence of the sintering process and changes in thecrystallographic and compositional structure of the tube. For example,binders within the composition may burn-out, leaving behind acarbonaceous reside on the outer surface of the tube. That carbonaceousresidue, generally in the form of free carbon, can negatively impact thequality of bond between the tube and the base component, inhibiting ahermetic seal.

Processing to form an extended length ceramic tube structure continueswith provision of an un-sintered or partially sintered ceramic couplingcomponent. That ceramic coupling component is arranged so as to overlieor circumscribe the first and second tube segments, particularly at thesecond end of the first tube segment and the first end of the secondtube segment, and more particularly at the portions on the first andsecond tube segments where they first and second tube segments meet eachother. Subsequently, the arrangement of the first and second tubesegments and the positioned coupling component is then subjected to asintering step during which the coupling component shrinks to its finaldimensions.

Further, before the pre-sintering step, each of the ceramic tubesegments may be subjected to a machining operation. Statedalternatively, this machining step is carried out in the green state,where the tube is in a state that allows easier material removal than inthe sintered state. The machining may be effective to reduce or evencompletely remove dimensional or surface irregularities of the greentube. For example, in the case of extrusion, the green tube may havecharacteristic score lines extending partially or wholly along theentire length of the tube. Those score lines can inhibit the formationof a strong interfacial sinter bond, as well as a hermetic seal. In thecase of other formation technologies, machining may still be desirable.For example, in the case of isopressing or molding, characteristicimperfections may be left behind on the green tube, such as flashing.

Sintered ceramic bodies of silicon carbide according to an embodimentmay be characterized by the amount the bodies shrink from a green stateto a fully sintered state. For example, green ceramic bodies of siliconcarbide according to an embodiment may shrink more than about 10% fromtheir original size, more than about 12%, more than about 15%, more thanabout 17%, less than about 25%, less than about 20%, less than about17%, less than about 15% upon being fully sintered. In a particularembodiment, a green ceramic body of silicon carbide may shrinkapproximately 17% from its original size upon being fully sintered. Whencombining a pre-sintered first component, such as a tube, with a greensecond component, such as an un-sintered or incompletely sinteredcoupling component that circumvents the pre-sintered first component,the shrinkage relationship, and the amount of interference bond, can beexpressed as follows.

ID _(c,FS) =OD _(p)−Δ, where

ID_(c,FS) is the inside diameter (ID) of a fully sintered couplingcomponent, OD_(t) is IDc,FS/(1−Rs)=IDc, where outside diameter, of 2.0″(i.e. OD_(t)=2.0). An interference bond of 5% (i.e. A=5%) of a secondbody, such as the coupling component, requires a fully sintered couplingcomponent ID (ID_(c,FS)) to be 0.10″ less than the OD_(t) (i.e.2.0*5%=0.10), or 1.90″ (i.e. ID_(c,FS)=OD_(t)−Δ, or 1.90″=2.0″−0.10″).Thus, to attain a 5% interference of a fully sintered coupling componenton the pre-sintered tube, the green coupling component will be made tohave a theoretically fully sintered inner diameter (if it were sinteredby itself) of 1.90″.

Further, the ID of the green second component (i.e. the un-sinteredcoupling component) can be expressed as follows.

ID _(c,FS)/(1−R _(s))=ID _(c), where

ID_(c) is the inner diameter of the green second component, orun-sintered coupling component, and R_(s) is the shrinkage rate of thesecond component (expressed as a decimal). Thus, in accordance with theexample given above, and assuming the shrinkage rate of the secondcomponent is 17.0%, the inner diameter of the green coupling component(ID_(c)) can be calculated as 1.9÷(1−0.170)=2.289″.

Turning to specific embodiments, a first embodiment of an extendedlength tube structure is shown in FIGS. 1 and 2. FIG. 1 is across-section of an extended length tube segment containing 3 segments,and FIG. 2 shows that same structure but in plan view. The extendedlength tube segment includes a first tube segment 14, a second tubesegment 12, and a third tube segment 10, each being arranged in end-endrelationship. As particularly shown in FIG. 1, the first tube segment 14includes a first end 15 and a second end 16. The second tube segment 12includes a first end 18. Further, the first and second couplingcomponents 22, 20, respectively are shown, and are disposed about theinterfaces between the second end 16 of the first component 14 and thefirst end 18 of the second component 12.

FIGS. 3 and 4 show different geometric configurations for the end facesof adjacent tube segments. FIG. 3 illustrates a simplified structurehaving a first tube segment 30, a second tube segment 35, the first tubesegment 30 having a planar end face 31, the second tube segment 35having a planar end face 36.

FIG. 4 illustrates what can be referred to as a “shiplapped” engagementstructure between adjacent tube segments, including a first tube segment40 having an L-shaped end face 41, and a second tube-segment 45 havingan L-shaped end face 46. As shown, the L-shaped structures are invertedwith respect to each other so as to be complementary in nature, andachieve a “keyed” configuration.

FIG. 5 is an SEM cross-section showing the interfacial bond between apre-sintered silicon carbide tube 50, and a base component, such as acoupling component, 52. Between the components 50 and 52 is an interface54, which provides a hermetic seal between components 50 and 52. Theinterface 54 may also be defined as a sinter bond (e.g. sintered bond)or an interference bond or fit. While the interface may be easily seenin the figure, it should be noted that portions of the interface areobscured by a non-colored or white depiction. These areas indicate areaswhere grain growth occurred across the interface (i.e. crystallographicgrains extend across and bridge, functioning to strengthen and enhancethe hermetic seal across the interface. Stated alternatively, grains,formed of crystals from each of the two components joined and grew orextended so as to bridge the interface creating a strong chemical orcrystallographic bond across the interface. Consequently, the bond ismore complex than a typical friction-fit direct bond structure, butincludes both mechanical and crystallographic components to improve therobustness of the interface.

The following examples include helium pressure testing on embodiments ofarticles having silicon carbide components including a sinter bond, orinterference bond, according to the embodiments discussed above. Theembodiments tested generally included a pre-sintered tube with a flange,cap, or other component sintered to the pre-sintered tube. Although thearticles and components tested may vary in some respects to thosedisclosed herein, the tested seals (e.g. interference bonds,sintered-bonds) in the following examples are similar or identical tothe embodiments of the seals described and disclosed herein, and thusthe results are relevant to the performance of the disclosedembodiments.

Example 1

Several ceramic articles were formed to include an interference bondbetween a ceramic tube and ceramic flange as follows. A 14 mm OD ceramictube was prepared according to the methods discussed above. One end ofthe tube was capped, and the tube and cap was pre-sintered according tothe methods discussed above in order to provide a pre-sintered tube witha closed end and an open end. Several green ceramic flanges wereprepared according to the methods above to fit over the open end of thepre-sintered tube. The green ceramic flanges were engineered to providea fully-sintered ID that was less than the OD of the 14 mm tube (e.g.interference) by about 0% to about 15%. The green ceramic flanges wereprovided on the open end of the pre-sintered tube and was co-sinteredwith the pre-sintered tube to provide an interference bond according tothe methods discussed above.

After the ceramic articles were formed, they were pressure tested byproviding 200 psi (about 13.8 bar) of helium (He) on one side of theinterference bond to determine the integrity of the interference bond ofeach ceramic article. FIG. 6 shows that the majority of the samples ofceramic articles having a flange engineered to have between about 0% toabout 5% fully-sintered ID failed in holding pressure. FIG. 6 also showsthat a majority of the sample of ceramic articles having a flangeengineered to have between about 5% to about 15% fully-sintered IDsucceeded in holding pressure. In particular, FIG. 6 tends to show thata threshold value of about 5% is successful in holding pressure.

Example 2

A ceramic article having a 100 mm OD tube was prepared and pre-sinteredaccording to the methods discussed above, and was fitted with a greenflange engineered to have a fully-sintered ID of 3% less than thepre-sintered tube. The tube and flange were co-sintered to form aceramic article having an interference bond according to the methodsdiscussed above, and pressure tested at 20° C. with 6 barg (bar gauge)of helium on one side of the interference bond to determine theintegrity of the interference bond of the ceramic article. The ceramicarticle lost about 0.2 bar over a 12 hour period.

Example 3

Three ceramic articles having a 35 mm OD tube were prepared andpre-sintered according to the methods discussed above, and each wasfitted with a green flange and subsequently co-sintered to form aceramic article having an interference bond according to the methodsdiscussed above. A first ceramic article included a flange engineered tohave a fully-sintered ID of 3% less than the pre-sintered tube, a secondceramic article included a flange engineered to have a fully-sintered IDof 5% less than the pre-sintered tube, and a third ceramic articleincluded a flange engineered to have a fully-sintered ID of 11% lessthan the pre-sintered tube. The three ceramic articles were subjected tofive (5) thermal cycles from 20° C. to 1000° C., and pressurized with 6barg of helium on one side of the interference bond to determine theintegrity of the interference bond of each ceramic article. Pressurereadings were taken at 20° C. and 1000° C. for each ceramic article ateach iteration of thermal cycling. The results of the 20° C. readingsare shown in FIG. 10, and the results for the 1000° C. are shown in FIG.11, where sample “A” is the 3% sample and depicted as a triangle, sample“B” is the 5% sample and depicted as a diamond, and sample “C” is the11% sample and depicted as a square.

As shown in FIG. 7, samples A and B lost less than 0.1 (−0.1) bar/H at20° C. The average pressure loss for sample A at 20° C. is less thanabout 0.03 bar/H, and the average pressure loss for sample B at 20° C.is less than about 0.01 bar/H. FIG. 10 also shows that sample Cincreasingly lost pressure at each thermal cycle reading taken at 20° C.It is unclear why sample C readings show a continuous loss in pressureas this is contrary to the expectations of that sample.

Turning to FIG. 8, sample A (the 3% sample) actually shows an increasein pressure at each thermal cycle reading taken at 1000° C. It isunclear why pressure increased in sample A at 1000° C. The averagepressure gain of sample A taken at 1000° C. is about 0.06 bar/H. In FIG.8, sample B (the 5% sample) shows less than 0.2 (−0.2) bar/H pressureloss. The average pressure loss for sample B taken at 1000° C. is lessthan about 0.03 bar/H. FIG. 8 also shows that sample C (the 11% sample)has a continuous increase in pressure loss at each thermal cycle, whichis consistent with the data of FIG. 7. The results of the thermal cyclepressure readings of FIGS. 7 and 8 tend to show that sample B (the 5%sample) provides a tighter interference bond than either sample A or C.

Example 4

A ceramic article was prepared according to sample B (the 5% sample) inExample 3 above, and was tested for pressure loss at intermediatetemperatures by pressurizing one side of the interference bond of theceramic article with 2 barg of helium while heating the ceramic articleup to 1000° C. As FIG. 9 shows, frequent measurements were taken atseveral temperatures between the thermal cycle of about 100° C. to about900° C. As FIG. 9 also indicates, the pressure in the tube (measured inbarg) remained between about 2 barg and 2.5 barg through the thermalcycle. The results of this example indicate little to no loss ordegradation of tightness in the interference bond throughout a thermalcycle, also suggesting that the secondary component (cap, flange, etc.)bonds well to the tube because both components have identical, or nearlyidentical, coefficients of thermal expansion (CTE). It is also notedthat, although not shown in the FIGS., several samples have been knownto operate at greater than about 1000° C., greater than about 1300° C.,and even greater than 2000° C. with no appreciable increase in pressureloss when subsequently tested at temperatures at or below 1000° C.

Example 5

Three ceramic articles (samples A, B, and C) were prepared according toexample 3 above, and subjected to five (5) testing iterations of thermalcycles between 20° C. and 1000° C. while provided with 6 barg of heliumon one side of the interference bond of each sample. The results areshown in FIGS. 10 and 11. As shown in FIG. 10, sample A (3% sample) hadan average pressure loss at 20° C. of about 0.05 bar/H, sample B (5%sample) had an average pressure loss at 20° C. of about 0.03 bar/h, andsample C (11% sample) had an average pressure loss of about 0.13 bar/H.FIG. 11 shows that sample B tends to provide a pressure increase at1000° C. It is unclear why sample B increases pressure in the tube at1000° C. However, FIGS. 10 and 11 appear to indicate that sample Bprovides the tightest interference bond and, thus, provides higherfidelity in pressure retention at thermal cycling than the othersamples.

Example 6

Three ceramic articles (samples A, B, and C) were prepared according toexample 3 above, and subjected to a long duration (about 72-80 hours)pressure test at 1000° C. with 6 barg of helium on one side of theinterference bond of each sample. The results of the long durationpressure test are shown in FIG. 12. As shown in FIG. 12, sample B (5%sample) lost all pressure at the end of the long duration test, atapproximately 72 hours. The results are anomalous, and it is believedthat a hermetic seal was not fully achieved with sample B.

What is claimed is:
 1. An extended length tube structure comprising: afirst ceramic tube segment having a first end and a second end; a secondceramic tube segment having a first end and a second end, the second endof the first ceramic tube segment being arranged to face the first endof the second ceramic tube segment, each of the first and second ceramictube segments having an inner diameter and an outer diameter; and aceramic coupling component sinter bonded to the second end of the firsttube segment and the first end of the second tube segment such that thefirst and second tube segments are arranged end to end to form acontinuous tube structure, wherein each of the ceramic tube segmentsforms a seal with the coupling component, wherein the seal has at leastone performance characteristic selected from the group consisting of: i)a Shear Strength not less than about 25 MPa; ii) a Nitrogen SealPerformance of not greater than 10%; iii) a Helium Seal Performance ofnot greater than 10%; iv) a Vacuum Seal Performance of not greater than10%.
 2. The extended length tube structure of claim 1, wherein thesecond end of the first ceramic tube segment is in abutting contact withthe first end of the second ceramic tube segment.
 3. The extended lengthtube structure of claim 1, wherein the second end of the first tubesegment has an end face and the first end of the second ceramic tubestructure has an end face, and wherein the end faces have complementarystructures.
 4. The extended length tube structure of claim 3, whereinthe end faces are planar.
 5. The extended length tube structure of claim3, wherein the end faces lie in a plane perpendicular to a longitudinalaxis of the first or second ceramic tube segment.
 6. The extended lengthtube structure of claim 1, wherein the extended length tube structurehas an outer diameter (OD) and a length (L), and an aspect ratio of L:ODof not less than about 10:1 and not greater than 300:1.
 7. The extendedlength tube structure of claim 1, wherein the first ceramic tubesegment, the second ceramic tube segment, the coupling component, or anycombination thereof comprises silicon carbide.
 8. The extended lengthtube structure of claim 7, wherein each of the first ceramic tubesegment, the second ceramic tube segment, the coupling componentcomprise silicon carbide.
 9. The extended length tube structure of claim8, wherein the silicon carbide comprises a content of the siliconcarbide from at least about 91 wt % to no greater than about 99.85 wt %,wherein at least about 95 wt % of the silicon carbide is alpha phase.10. The extended length tube structure of claim 9, wherein the siliconcarbide further comprises: a carbonized organic material in an amount nogreater than about 5.0 wt %; boron in an amount from at least about 0.15wt % to no greater than about 3.0 wt %; additional carbon in an amountno greater than about 1.0 wt %; and a predominantly equiaxedmicrostructure.
 11. The extended length tube structure of claim 1,wherein the first tube segment, the second tube segment, and thecoupling component are coaxial.
 12. The extended length tube structureof claim 1, wherein the coupling component comprises a cylindrical body.13. The extended length tube structure of claim 1, whereincrystallographic grains from each of the first tube segment and thecoupling component extend across and bridge a sinter bond interfacebetween the first tube segment and the coupling component, and whereincrystallographic grains from each of the second tube segment and thecoupling component extend across and bridge a sinter bond interfacebetween the first tube segment and the coupling component.
 14. Theextended length tube structure of claim 1, wherein at least one of theseals has a Shear Strength of not less than about 40 MPa.
 15. Theextended length tube structure of claim 1, wherein the seal is ahermetic seal.
 16. A method of forming an extended length ceramic tubestructure, comprising: providing a first ceramic tube segment having afirst end and a second end, providing a second ceramic tube segmenthaving a first end and a second end; pre-sintering the first and secondceramic tube segments; surface cleaning an outer surface of each of thetube segments; providing an un-sintered or partially sintered ceramiccoupling component; arranging the first and second tube segments and thecoupling component such that the second end of the first ceramic tubesegment faces the first end of the second ceramic tube segment, and thecoupling component overlies the second end of the first tube segment andthe first end of the second tube segment; and co-sintering the first andsecond tube segments and the coupling component to form a seal betweenthe coupling component and each of the first and second tube segments.17. The method of claim 16, further comprising: forming crystallographicgrains from each of the first tube segment and the coupling componentsuch that the crystallographic extend across and bridge an interfacedefined by the seal between the first tube segment and the couplingcomponent, and forming crystallographic grains from each of the secondtube segment and the coupling component such that the crystallographicgrains extend across and bridge an interface defined by the seal betweenthe first tube segment and the coupling component.
 18. The method ofclaim 16, wherein the second end of the first ceramic tube segment is inabutting contact with the first end of the second ceramic tube segments.19. The method of claim 16, wherein the second end of the first tubesegment has an end face, and the first end of the second ceramic tubestructure has an end face, wherein the end faces have complementarystructures.
 20. The method of claim 16, wherein the first ceramic tubesegment, the second ceramic tube segment, the coupling component, or anycombination thereof comprises silicon carbide.